CN107955303A - Compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide and preparation method thereof - Google Patents

Compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide and preparation method thereof Download PDF

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Publication number
CN107955303A
CN107955303A CN201711181990.3A CN201711181990A CN107955303A CN 107955303 A CN107955303 A CN 107955303A CN 201711181990 A CN201711181990 A CN 201711181990A CN 107955303 A CN107955303 A CN 107955303A
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polyvinyl alcohol
nano
titanium dioxide
adds
distilled water
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吴祥忠
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DANGTU COUNTY RUILONG FRUIT TREE PLANTING PROFESSIONAL COOPERATIVES
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DANGTU COUNTY RUILONG FRUIT TREE PLANTING PROFESSIONAL COOPERATIVES
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/07—Aldehydes; Ketones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds

Abstract

The invention discloses a kind of compound anti-ultraviolet degradable polyvinyl alcohol preservative film of nano-titanium dioxide, and its preparation process, it is characterized in that, with polyvinyl alcohol, bentonite, citric acid, glycerine, gluconic acid, carbon black, polyetheramine, nano silicon dioxide, neopelex, potassium hydroxide, graphene oxide, carbon nanotubes, pentanediol, acetic acid, nano-titanium dioxide, triethanolamine, KH550 etc. for raw material.Bentonite reacts with gluconic acid in the present invention, and intermolecular hydrogen bonding is formd with polyvinyl alcohol, improves its water resistance.Graphene oxide (GO) passes through Hydrogenbond, the mechanical property of raising PVA materials between PVA；Carbon nanotubes is handled with neopelex, potassium hydroxide, improves its tensile strength；With glutaraldehyde as cross linker, using acetic acid as catalyst, intermolecular acetalation crosslinking can occur for PVA, improve its water resistance.

Description

A kind of compound anti-ultraviolet degradable polyvinyl alcohol of nano-titanium dioxide is fresh-keeping Film and preparation method thereof
Technical field
The present invention relates to field of compound material, and in particular to a kind of compound anti-ultraviolet degradable of nano-titanium dioxide Type polyvinyl alcohol preservative film, and its preparation process.
Background technology
With the raising of public life level, people increasingly pay attention to for food security and Environmental security so that tradition Plastic fresh-keeping membrane enjoys query.So, the security and shelf life of food how are ensured, at the same it is again environmentally friendly, how to make Standby edible or degradable preservative film, becomes industry research and the important directions of development.
Yellow Hui honor is in its master thesis《The preparation of bentonite/PVA preservative films and its application in mango fresh-keeping are ground Study carefully》In one text, using bentonite as packing material, with polyvinyl alcohol（PVA）For base material, bentonite and its load chemical assistant are studied （Citric acid）Suction-operated of the Perserving materials to ethene.Bentonite, glycerine, citric acid are added to the water, stirs, adds poly- second Enol, is warming up to 90 DEG C of water-baths insulation, and ultrasound, excludes bubble, be cooled to room temperature, be poured on poly (methyl methacrylate) plate, with scraping cutter painting Cloth forms a film, and film is stood 24h at room temperature, makes moisture evaporation, then film is placed in 45 DEG C of vacuum drying chamber again dry 24h, is made bentonite/PVA preservative films.But there are mechanical property, water resistance deficiency.
Bentonite reacts with gluconic acid in the present invention, obtains the material for having hydroxyl modified to surface, with polyvinyl alcohol Intermolecular hydrogen bonding is formd, there is good compatibility, improve its water resistance.With polyethex amine modification carbon black, nano silicon dioxide The reinforcement with core shell structure is obtained, hydrogen bond is formed between the amido and PVA on modified carbon black surface, is tightly combined, is improved multiple The mechanical property of condensation material, while reduce the hydroscopicity of material；Nano silicon dioxide plays thickening power to polyetheramine, in PVA Favorable dispersibility in film, improves the tensile strength of composite membrane.Graphene oxide (GO) is dispersed good in PVA matrixes Good, between the two by Hydrogenbond, the addition of GO improves the mechanical property of PVA materials；With neopelex, hydrogen Potassium oxide handles carbon nanotubes, improves its dispersiveness, tensile strength.With glutaraldehyde as cross linker, using acetic acid as catalysis Agent, PVA can occur intermolecular acetalation crosslinking, be prepared for Modified Membrane using acetal cross-linking method, improve its water resistance.
The content of the invention
The invention mainly solves the technical problem of providing a kind of compound anti-ultraviolet degradable of nano-titanium dioxide Type polyvinyl alcohol preservative film and its preparation process, the preservative film degradability made according to the technique, waterproof is water-fast, mechanical property Good, uvioresistant.
The technical problems to be solved by the invention are realized using following technical solution：
Polyvinyl alcohol 30-43, bentonite 5-12, citric acid 6-10, glycerine 2-4, gluconic acid 3-7, carbon black 4-6, polyetheramine 5- 9, nano silicon dioxide 5-8, neopelex 2-5, potassium hydroxide 3-6, graphene oxide 4-7, carbon nanotubes 7-10, Pentanediol 4-6, acetic acid 3-5, nano-titanium dioxide 4-8, triethanolamine 3-7, KH550 2-6, ethanol, H2SO4, distilled water.
A kind of preparation method of the compound anti-ultraviolet degradable polyvinyl alcohol preservative film of nano-titanium dioxide, it is special Sign is, carries out according to the following steps：
A. bentonite, glycerine are mixed, 1:10-20 adds distilled water, and stirring 1-2h is uniformly dispersed, and tune pH is 7-8, and 1:5-10 Citric acid, ethanol are added, is warming up to 70-80 DEG C of water bath with thermostatic control, gluconic acid is slowly added dropwise, stirring reaction 3-4h, filters, washing Alcohol is washed 3-5 times, and 30-50 DEG C of vacuum drying, crush, cross 100-200 mesh sieves；
B. into carbon black 1:3-5 adds dense H2SO4, magnetic agitation 1-2h, 70-80 DEG C of ultrasound 2-3h, obtains A liquid, by polyetheramine, Nano silicon dioxide 1:10-20 is scattered in distilled water, is added drop-wise in A liquid, and after magnetic agitation 4-8h, 60-70 DEG C of drying, is treated With；
C. by neopelex, potassium hydroxide 1:15-25 is dissolved in distilled water, adds carbon nanotubes, graphite oxide Alkene, is warming up to 85-95 DEG C of sonic oscillation 4-5h, filtering, washing 3-5 times, 50-60 DEG C of vacuum drying；
D. by nano-titanium dioxide 70-80 DEG C be heat-treated 5-8h, 1:20-30 adds distilled water, is dispersed with stirring, and adds three second Hydramine, 1:5-10 adds KH550, ethanol, is warming up to 75-85 DEG C, and tune pH is 8-9, the lower reaction 1-2h of ultrasound, centrifugation, 80-90 DEG C It is dry complete, obtain modified powder；
E. into polyvinyl alcohol 1:20-30 adds distilled water, is heated to 80-90 DEG C of stirring and dissolving, adds gained in a, b, c, d Material and pentanediol, acetic acid, ultrasonic 1-2h are sufficiently mixed, and constant temperature stirring reaction 1-2h, excludes bubble, be cooled to room temperature, topple over On poly (methyl methacrylate) plate, formed a film with scraper for coating, film is stood into 6-10h at room temperature, makes moisture evaporation, then film is placed in 45- Dry 5-10h, is made a kind of polyvinyl alcohol preservative film in 55 DEG C of vacuum drying chamber.
The reaction mechanism of the present invention is as follows：
（1）Bentonite reacts with gluconic acid, obtains the material for having hydroxyl modified to surface, and molecule is formd with polyvinyl alcohol Between hydrogen bond, there is good compatibility, improve its water resistance.
（2）The reinforcement with core shell structure, modified carbon black surface are obtained with polyethex amine modification carbon black, nano silicon dioxide Amido and PVA between form hydrogen bond, be tightly combined, improve the mechanical property of composite material, while reduce the moisture absorption of material Rate；Nano silicon dioxide plays thickening power to polyetheramine, the favorable dispersibility in PVA film, improves the stretching of composite membrane Intensity.
（3）Favorable dispersibility of the graphene oxide (GO) in PVA matrixes, between the two by Hydrogenbond, GO's adds Enter to improve the mechanical property of PVA materials；Carbon nanotubes is handled with neopelex, potassium hydroxide, is improved Its dispersiveness, tensile strength.
（4）With glutaraldehyde as cross linker, using acetic acid as catalyst, intermolecular acetalation crosslinking can occur for PVA, use Acetal cross-linking method is prepared for Modified Membrane, improves its water resistance.
Embodiment
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment
The compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide, by following weight parts (g) raw material is made：
Polyvinyl alcohol 43, bentonite 12, citric acid 10, glycerine 4, gluconic acid 7, carbon black 6, polyetheramine 9, nano silicon dioxide 8, Neopelex 5, potassium hydroxide 6, graphene oxide 7, carbon nanotubes 10, pentanediol 6, acetic acid 5, nano-titanium dioxide 8, triethanolamine 7, KH550 6, ethanol, H2SO4, distilled water.
A kind of preparation method of the compound anti-ultraviolet degradable polyvinyl alcohol preservative film of nano-titanium dioxide, it is special Sign is, carries out according to the following steps：
A. bentonite, glycerine are mixed, 1:20 add distilled water, and stirring 2h is uniformly dispersed, and tune pH is 7-8, and 1:10 add lemon Acid, ethanol, are warming up to 70-80 DEG C of water bath with thermostatic control, and gluconic acid, stirring reaction 3h is slowly added dropwise, and suction filtration, washing alcohol are washed 3 times, 40-50 DEG C of vacuum drying, crush, cross 100 mesh sieves；
B. into carbon black 1:5 add dense H2SO4, magnetic agitation 1h, 70-80 DEG C of ultrasound 2h, obtains A liquid, by polyetheramine, nanometer two Silica 1:20 are scattered in distilled water, are added drop-wise in A liquid, and after magnetic agitation 4h, 60-70 DEG C of drying is stand-by；
C. by neopelex, potassium hydroxide 1:25 are dissolved in distilled water, add carbon nanotubes, graphene oxide, rise Temperature is to 85-95 DEG C of sonic oscillation 4h, and filtering, washing 3 times, 50-60 DEG C is dried in vacuo；
D. by nano-titanium dioxide 70-80 DEG C be heat-treated 5h, 1:30 add distilled water, are dispersed with stirring, addition triethanolamine, 1:10 add KH550, ethanol, are warming up to 75-85 DEG C, and tune pH is 8-9, and the lower reaction 2h of ultrasound, centrifugation, 80-90 DEG C of drying is complete, Obtain modified powder；
E. into polyvinyl alcohol 1:25 add distilled water, are heated to 80-90 DEG C of stirring and dissolving, add resulting material in a, b, c, d And pentanediol, acetic acid, ultrasonic 2h are sufficiently mixed, constant temperature stirring reaction 2h, excludes bubble, is cooled to room temperature, is poured over organic glass In glass plate, formed a film with scraper for coating, film is stood into 10h at room temperature, makes moisture evaporation, then film is placed in 45-55 DEG C of vacuum Dry 8h, is made a kind of polyvinyl alcohol preservative film in drying box.
The compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide prepared by above-described embodiment Performance test results are as follows：
Tensile strength >=65.2MPa, tearing strength >=96.4MPa, elongation at break >=149.3%, can extend fruit goods under room temperature Frame phase 2-4d, the lower shelf life 5-8d that can extend fruit of refrigeration.

Claims (2)

1. the compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide, it is characterised in that under The raw material for stating parts by weight is made：
Polyvinyl alcohol 30-43, bentonite 5-12, citric acid 6-10, glycerine 2-4, gluconic acid 3-7, carbon black 4-6, polyetheramine 5- 9, nano silicon dioxide 5-8, neopelex 2-5, potassium hydroxide 3-6, graphene oxide 4-7, carbon nanotubes 7-10, Pentanediol 4-6, acetic acid 3-5, nano-titanium dioxide 4-8, triethanolamine 3-7, KH550 2-6, ethanol, H2SO4, distilled water.
2. a kind of compound anti-ultraviolet degradable polyvinyl alcohol of nano-titanium dioxide according to claim 1 is fresh-keeping The preparation method of film, it is characterised in that carry out according to the following steps：
A. bentonite, glycerine are mixed, 1:10-20 adds distilled water, and stirring 1-2h is uniformly dispersed, and tune pH is 7-8, and 1:5-10 Citric acid, ethanol are added, is warming up to 70-80 DEG C of water bath with thermostatic control, gluconic acid is slowly added dropwise, stirring reaction 3-4h, filters, washing Alcohol is washed 3-5 times, and 30-50 DEG C of vacuum drying, crush, cross 100-200 mesh sieves；
B. into carbon black 1:3-5 adds H2SO4, magnetic agitation 1-2h, 70-80 DEG C of ultrasound 2-3h, obtains A liquid, by polyetheramine, nanometer Silica 1:10-20 is scattered in distilled water, is added drop-wise in A liquid, and after magnetic agitation 4-8h, 60-70 DEG C of drying is stand-by；
C. by neopelex, potassium hydroxide 1:15-25 is dissolved in distilled water, adds carbon nanotubes, graphite oxide Alkene, is warming up to 85-95 DEG C of sonic oscillation 4-5h, filtering, washing 3-5 times, 50-60 DEG C of vacuum drying；
D. by nano-titanium dioxide 70-80 DEG C be heat-treated 5-8h, 1:20-30 adds distilled water, is dispersed with stirring, and adds three second Hydramine, 1:5-10 adds KH550, ethanol, is warming up to 75-85 DEG C, and tune pH is 8-9, the lower reaction 1-2h of ultrasound, centrifugation, 80-90 DEG C It is dry complete, obtain modified powder；
E. into polyvinyl alcohol 1:20-30 adds distilled water, is heated to 80-90 DEG C of stirring and dissolving, adds gained in a, b, c, d Material and pentanediol, acetic acid, ultrasonic 1-2h are sufficiently mixed, and constant temperature stirring reaction 1-2h, excludes bubble, be cooled to room temperature, topple over On poly (methyl methacrylate) plate, formed a film with scraper for coating, film is stood into 6-10h at room temperature, makes moisture evaporation, then film is placed in 45- Dry 5-10h, is made a kind of polyvinyl alcohol preservative film in 55 DEG C of vacuum drying chamber.
CN201711181990.3A 2017-11-23 2017-11-23 Compound anti-ultraviolet degradable polyvinyl alcohol preservative film of a kind of nano-titanium dioxide and preparation method thereof Withdrawn CN107955303A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108752694A (en) * 2018-06-01 2018-11-06 安徽永豪日用品有限公司 A kind of polyethylene preservative film with good tensile strength
CN108786792A (en) * 2018-06-25 2018-11-13 福州大学 A kind of metal/semiconductor composite photo-catalyst and its preparation and application
CN113201177A (en) * 2021-04-09 2021-08-03 广西壮族自治区农业科学院 Nano freshness protection package material and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105907008A (en) * 2016-05-03 2016-08-31 四川农业大学 Antibacterial plastic wrap and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105907008A (en) * 2016-05-03 2016-08-31 四川农业大学 Antibacterial plastic wrap and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108752694A (en) * 2018-06-01 2018-11-06 安徽永豪日用品有限公司 A kind of polyethylene preservative film with good tensile strength
CN108786792A (en) * 2018-06-25 2018-11-13 福州大学 A kind of metal/semiconductor composite photo-catalyst and its preparation and application
CN108786792B (en) * 2018-06-25 2021-03-26 福州大学 Metal/semiconductor composite photocatalyst and preparation and application thereof
CN113201177A (en) * 2021-04-09 2021-08-03 广西壮族自治区农业科学院 Nano freshness protection package material and preparation method and application thereof

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